CN1743276A - Lithium cell anode material lithium manganate preparing method - Google Patents
Lithium cell anode material lithium manganate preparing method Download PDFInfo
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- CN1743276A CN1743276A CNA2004100736721A CN200410073672A CN1743276A CN 1743276 A CN1743276 A CN 1743276A CN A2004100736721 A CNA2004100736721 A CN A2004100736721A CN 200410073672 A CN200410073672 A CN 200410073672A CN 1743276 A CN1743276 A CN 1743276A
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Abstract
This method provides a preparation method for lithium manganate powder which is used as anode material of lithium ion cell. This method includes: first, use a water soluble macromolecule polymer as dispersant/gelatinizer to prepare 0.2~20g/100ml concentration aqueous solution which is used as solvent in the next step; then add water soluble lithium ion compound to the solvent to acquire 0.05~2 mol/L lithium-concentration lithium solution; next, add solid MnO2 powder in mol ratio of (0.8~1.2) ~2 into the obtained lithium solution agitating meanwhile, then evaporate water to get gelinite, in the end, roast the gelinite under 300~850 deg.C for 0.7~28 hours. Advantages: homogeneous grains, high first-charge-discharge efficiency, high reversible-ratio capacity and excellent cycle performance.
Description
[technical field]
The present invention relates to lithium-ion secondary cell, be specifically related to a kind of preparation method of positive-material lithium manganate of lithium-ion secondary cell.
[background technology]
The positive electrode material of commercialization lithium ion battery mainly is cobalt acid lithium (LiCoO
2), since rare, the expensive price of cobalt resource with and toxicity to the influence of environment, limited its development potentiality.Another kind of positive electrode material lithium nickelate (LiNiO
2) though price is lower, better performances, preparation is complicated and have a high temperature safety problem.Lithium manganate (the LiMn of spinel structure by contrast
2O
4) because manganese material is abundant and cheap, and nontoxic, pollutes little, easily recovery, the operating voltage height, it is big to take off the lithium amount, and advantage such as safety performance is good, becomes the anode material for lithium-ion batteries of being paid close attention to.
The preparation method of lithium manganate mostly adopts solid-phase synthesis.For example, CN1455466A discloses the preparation method of a kind of lithium ion battery with constitutionally stable spinel lithium manganate, be that the electrolytic manganese dioxide of particle diameter 10～20 μ m, the Quilonum Retard of particle diameter 5～10 μ m and the cobalt oxide of particle diameter 5～10 μ m are mixed, form through multi-element doping, high temperature solid-phase sintering.The advantage of this solid-phase synthesis is that technology is simple, but also has obvious defects: the composition of synthetic materials is inhomogeneous, and particle size distribution is wide and form is irregular, thereby has influenced the battery performance of material.
[summary of the invention]
Purpose of the present invention is exactly in order to overcome above-mentioned the deficiencies in the prior art, and a kind of preparation method of anode material for lithium ion battery lithium manganate is provided.
The preparation method of a kind of lithium cell anode material lithium manganate that the present invention proposes is characterized in that comprising the following steps:
(1) will be mixed with the aqueous solution that concentration is 0.2～20g/100ml as a kind of high molecular weight water soluble polymer of dispersion/jelling agent, with this as solvent;
(2) add water-soluble lithium ion compound in step (1) gained solvent, being mixed with lithium concentration is the lithium solution of 0.05～2mol/L;
(3) stir down in step (2) gained lithium solution in Li: the Mn mol ratio is (0.8～1.2): 2 ratio adding MnO
2Pressed powder, transpiring moisture obtains gelinite then;
(4) gelinite that step (3) is obtained obtains to have the lithium manganate material of spinel structure 300～850 ℃ of roastings 0.7～28 hour.
In the method according to the invention, the described high molecular weight water soluble polymer of step (1) is mainly as reaction raw materials especially MnO
2The dispersion agent of pressed powder, and the jelling agent when forming gel as step (3).Can use as the high molecular weight water soluble polymer that described dispersion agent and jelling agent work, be selected from polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide, at least a in tetrafluoroethylene, the carboxymethyl cellulose partially but be preferably.The concentration of high molecular weight water soluble polymer in the described aqueous solution is preferably 0.2～20g/100ml described in the step (1), more preferably 1～15g/100ml; When this concentration was too low, dispersion effect was bad and/or need moisture evaporated too many when being difficult in step (3) to form gel or forming gel; When this concentration is too high, can increase cost on the one hand, also may have disadvantageous effect to dispersion effect on the other hand, and can produce pollution and influence product performance in the calcination steps afterwards.
In the method according to the invention, the described water-soluble lithium ion compound of step (2) can be lithium nitrate, lithium hydroxide, Quilonum Retard or Lithium Acetate, and they can use separately, also can be used in combination.
In the method according to the invention, described step (3) comprising: add MnO in described ratio under stirring in step (2) gained lithium solution
2Pressed powder, stirring at normal temperature stirred and are warming up to 50～90 ℃ after 1～4 hour, continued to stir transpiring moisture to forming gel under this temperature, placed 80～200 ℃ of warm airs to solidify then 1～24 hour, obtained gelinite.Described Li: the Mn mol ratio is preferably (0.8～1.2): 2, and more preferably about stoichiometry (Li: Mn mol ratio=1: 2).The MnO that is adopted
2The pressed powder raw material has no particular limits, and for example can be electrolytic process manganese dioxide powder or chemical method manganese dioxide powder or any other commodity manganese dioxide powder.
In the method according to the invention, comprised in 0.7～28 hour 300～850 ℃ of roastings at the gelinite that described in the step (4) step (3) is obtained: the heat-up rate with 0.5-10 ℃/min rises to 300～500 ℃ of constant temperature 0.2～4 hour earlier, heat-up rate with 0.5-10/min rises to 600～850 ℃ of constant temperature 0.5～24 hour again, is cooled to room temperature then.
In the method according to the invention, in the described lithium solution of step (2), also optionally contain Co
2+, Cr
3+, Al
3+, Ni
2+In the ion one or more.When adding these doped elements, its adding proportion (mol ratio) can be respectively: Co/Mn=0.03～0.1, Cr/Mn=0.01～0.05, Al/Mn=0.005～0.02, and/or Ni/Mn=0.01～0.05.These doped elements can join with the form of acetate or nitrate in the described lithium solution of step (2).
Among the preparation method of lithium cell anode material lithium manganate of the present invention, lithium salts is dissolved in the water, the polymer organic polymer is as dispersion agent, behind transpiring moisture, form gel, make reactant lithium ion and Manganse Dioxide in reaction medium, be in homodisperse state, thereby make the high temperature solid state reaction of follow-up lithium ion and Manganse Dioxide carry out more all even thoroughly, the product crystal formation that obtains is good, the purity height, chemical constitution is even, narrow diameter distribution, particle is more regular, and better electrochemical performance is arranged.By the doping of other element (cobalt, chromium, nickel, aluminium), can further improve the cyclical stability of material.
The present invention compared with prior art has the following advantages: the lithium manganate material that makes according to the inventive method has perfect spinel structure, narrow diameter distribution, and particle is regular; Gained lithium manganate material chemical property is good, product specific storage height, good cycle.
[description of drawings]
Fig. 1 is X-ray diffraction (XRD) figure of embodiment 1 gained lithium manganate material;
Fig. 2 is the electron scanning micrograph of embodiment 1 gained lithium manganate material;
Fig. 3 is the electron scanning micrograph of Comparative Examples 1 gained lithium manganate material.
[embodiment]
The present invention will be further described below in conjunction with embodiment, but these embodiment can not be interpreted as it is qualification to protection domain of the present invention.
In each embodiment and Comparative Examples, for the chemical property of the prepared positive electrode material of the preparation method who tests employing anode material for lithium-ion batteries of the present invention, with the LiMn that makes in each embodiment and the Comparative Examples
2O
4Material mixes the furnishing pulpous state with polyfluortetraethylene of binding element (PTFE) and deionized water and stirring, is coated in aluminium foil surface, makes the positive pole of lithium-ion secondary cell, and counter electrode is a metal lithium sheet, and electrolytic solution is 1MLiPF
6/ EC+DEC (1: 1) is assembled into button cell and tests.When test, charging and discharging currents density is 0.05mA/cm
2, at 3.3～4.2V voltage range internal recycle.Wherein measuring the method that first discharge specific capacity adopts is: the data of loading capacity first that experiment is recorded are divided by the quality of active material lithium manganese oxygen in the pole piece, and specific discharge capacity is first discharged.
Unless otherwise indicated, the raw material that uses in each embodiment and the Comparative Examples is analytical pure commercial chemistry reagent.
Embodiment 1
2 gram polyvinyl alcohol are dissolved in the 100ml water, add 4.279 gram LiOHH
2O makes its dissolving, stirs to add 17.388 gram MnO down
2(analytical pure commercial chemistry reagent, electrolytic process preparation, down with), restir is warming up to 80 ℃ of evaporation moisture content after 2 hours, stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 120 ℃ of baking ovens and solidifies 6 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 400 ℃ with 10 ℃/min, constant temperature 0.5 hour rises to 800 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 12 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 123.9mAh/g, and capability retention is 88.1% after 100 weeks of circulation.
Embodiment 2
8 gram polyoxyethylene glycol are dissolved in the 80ml water, add 3.695 gram Li
2CO
3Make its dissolving, stir the 17.388 gram MnO of adding down
2, restir is warming up to 70 ℃ of evaporation moisture content after 4 hours, and stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 120 ℃ of baking ovens and solidifies 3 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 400 ℃ with 5 ℃/min, constant temperature 0.5 hour rises to 700 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 12 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 120.6mAh/g, and capability retention is 88.4% after 100 weeks of circulation.
Embodiment 3
4 gram polyacrylamides are dissolved in the 1000ml water, add 7.240 gram LiNO
3Make its dissolving, stir the 17.388 gram MnO of adding down
2, restir is warming up to 80 ℃ of evaporation moisture content after 4 hours, and stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 150 ℃ of baking ovens and solidifies 4 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 450 ℃ with 10 ℃/min, constant temperature 0.5 hour rises to 800 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 12 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 126.2mAh/g, and capability retention is 86.6% after 100 weeks of circulation.
Embodiment 4
The poly-inclined to one side tetrafluoroethylene of 1 gram is dissolved in the 100ml water, adds 4.195 gram LiAc, add 0.005mol Cr (NO again
3)
3With 0.008mol Ni (NO
3)
2, after the dissolving evenly, stir the 17.388 gram MnO of adding down
2, restir is warming up to 60 ℃ of evaporation moisture content after 2 hours, and stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 100 ℃ of baking ovens and solidifies 12 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 500 ℃ with 10 ℃/min, constant temperature 0.5 hour rises to 750 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 16 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 118.7mAh/g, and capability retention is 85.1% after 100 weeks of circulation.
Embodiment 5
1 gram carboxymethyl cellulose is dissolved in the 100ml water, adds 4.195 gram LiOHH
2O adds 0.01mol CoAc again
2, after the dissolving evenly, stir the 17.388 gram MnO of adding down
2, restir is warming up to 80 ℃ of evaporation moisture content after 2 hours, and stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 120 ℃ of baking ovens and solidifies 6 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 400 ℃ with 10 ℃/min, constant temperature 0.5 hour rises to 800 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 12 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 129.8mAh/g, and capability retention is 89.2% after 100 weeks of circulation.
Embodiment 6
5 gram polyvinyl alcohol are dissolved in the 100ml water, add 4.195 gram LiOHH
2O adds 0.1875 gram Al (NO again
3)
29H
2O after the dissolving evenly, stirs the 17.388 gram MnO of adding down
2, restir is warming up to 80 ℃ of evaporation moisture content after 2 hours, and stirring-granulating always in this process stops to stir to fast evaporate to dryness moisture content, is put in 120 ℃ of baking ovens and solidifies 6 hours.The gelinite that obtains is placed in the alumina crucible, put into high temperature resistance furnace, rise to 400 ℃ with 10 ℃/min, constant temperature 0.5 hour rises to 790 ℃ with 5 ℃/min again, and constant temperature is furnace cooling after 12 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 116.6mAh/g, and capability retention is 85.5% after 100 weeks of circulation.
Comparative Examples 1
With 4.195 gram LiOHH
2O and 17.388 gram MnO
2Mixing in mortar, ball milling mixes compressing tablet after 2 hours again, and the compound that obtains is placed in the alumina crucible, puts into high temperature resistance furnace, rises to 800 ℃ with 10 ℃/min, and constant temperature is furnace cooling after 24 hours, obtains manganate cathode material for lithium.This positive electrode material and lithium counter electrode are assembled into button cell.The first discharge specific capacity that records battery is 104.3mAh/g, and capability retention is 80.7% after 100 weeks of circulation.
From the result of the foregoing description and Comparative Examples as can be seen, method provided by the invention is compared with traditional solid-phase synthesis, the gained lithium manganate material has perfect spinel structure, size distribution is narrower, particle is more regular, and the chemical property of gained lithium manganate material is better, product specific storage height, good cycle.
Claims (8)
1, a kind of preparation method of lithium cell anode material lithium manganate is characterized in that this method comprises the following steps:
(1) will be mixed with the aqueous solution that concentration is 0.2～20g/100ml as a kind of high molecular weight water soluble polymer of dispersion/jelling agent, with this as solvent;
(2) add water-soluble lithium ion compound in step (1) gained solvent, being mixed with lithium concentration is the lithium solution of 0.05～2mol/L;
(3) stir down in step (2) gained lithium solution in Li: the Mn mol ratio is (0.8～1.2): 2 ratio adding MnO
2Pressed powder, transpiring moisture obtains gelinite then;
(4) gelinite that step (3) is obtained obtains to have the lithium manganate material of spinel structure 300～850 ℃ of roastings 0.7～28 hour.
2, according to the process of claim 1 wherein that the described high molecular weight water soluble polymer of step (1) is to be selected from polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide, at least a in tetrafluoroethylene, the carboxymethyl cellulose partially.
3, according to the process of claim 1 wherein that the concentration of high molecular weight water soluble polymer in the described aqueous solution is 1～15g/100ml described in the step (1).
4, according to the process of claim 1 wherein that the described water-soluble lithium ion compound of step (2) is lithium nitrate, lithium hydroxide, Quilonum Retard or Lithium Acetate.
5, according to the process of claim 1 wherein that described step (3) comprising: in step (2) gained lithium solution, add MnO under stirring in described ratio
2Pressed powder, stirring at normal temperature stirred and are warming up to 50～90 ℃ after 1～4 hour, continued to stir transpiring moisture to forming gel under this temperature, placed 80～200 ℃ of warm airs to solidify then 1～24 hour, obtained gelinite.
6, according to the method for claim 1, wherein the gelinite that described in the step (4) step (3) is obtained comprised 300～850 ℃ of roastings in 0.7～28 hour: the heat-up rate with 0.5-10 ℃/min rises to 300～500 ℃ of constant temperature 0.2～4 hour earlier, heat-up rate with 0.5-10/min rises to 600～850 ℃ of constant temperature 0.5～24 hour again, is cooled to room temperature then.
7, be selected from Co according to the process of claim 1 wherein in the described lithium solution of step (2), optionally to contain
2+, Cr
3+, Al
3+, Ni
2+One or more doped elements in the ion.
8, method according to Claim 8, the interpolation mol ratio of wherein said doped element is respectively: Co/Mn=0.03～0.1, Cr/Mn=0.01～0.05, Al/Mn=0.005～0.02, and/or Ni/Mn=0.01～0.05.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101764211B (en) * | 2009-10-14 | 2012-10-03 | 青岛乾运高科新材料股份有限公司 | Preparation method of spherical lithium manganese for lithium-ion battery cathode material |
| CN103011299A (en) * | 2012-12-13 | 2013-04-03 | 青岛乾运高科新材料股份有限公司 | Preparation method of lithium manganate positive material |
| CN103187564A (en) * | 2011-12-28 | 2013-07-03 | 上海空间电源研究所 | Preparation method for battery anode material LiNi0.5Mn1.5O4 |
| CN103490056A (en) * | 2013-09-24 | 2014-01-01 | 四川国理锂材料有限公司 | Method for producing lithium manganate as lithium battery cathode material through wet mixing |
| CN106207156A (en) * | 2016-07-15 | 2016-12-07 | 新疆大学 | A kind of solid phase combustion prepares the method for big multiplying power LiMn2O4/graphite oxide composite |
| CN108736009A (en) * | 2018-05-29 | 2018-11-02 | 中伟新材料有限公司 | Cobalt nickel lithium manganate ternary material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326232A (en) * | 2000-05-25 | 2001-12-12 | 中国科学院成都有机化学研究所 | Process for preparing lithium manganese oxide as positive electrode of lithium ion battery |
| CN1472830A (en) * | 2003-06-05 | 2004-02-04 | 上海交通大学 | Anode material of lithium ion battery and preparing method thereof |
-
2004
- 2004-08-31 CN CNB2004100736721A patent/CN100436333C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101764211B (en) * | 2009-10-14 | 2012-10-03 | 青岛乾运高科新材料股份有限公司 | Preparation method of spherical lithium manganese for lithium-ion battery cathode material |
| CN103187564A (en) * | 2011-12-28 | 2013-07-03 | 上海空间电源研究所 | Preparation method for battery anode material LiNi0.5Mn1.5O4 |
| CN103011299A (en) * | 2012-12-13 | 2013-04-03 | 青岛乾运高科新材料股份有限公司 | Preparation method of lithium manganate positive material |
| CN103490056A (en) * | 2013-09-24 | 2014-01-01 | 四川国理锂材料有限公司 | Method for producing lithium manganate as lithium battery cathode material through wet mixing |
| CN103490056B (en) * | 2013-09-24 | 2015-11-25 | 四川国理锂材料有限公司 | Material by wet type mixing produces the method for anode material of lithium battery LiMn2O4 |
| CN106207156A (en) * | 2016-07-15 | 2016-12-07 | 新疆大学 | A kind of solid phase combustion prepares the method for big multiplying power LiMn2O4/graphite oxide composite |
| CN108736009A (en) * | 2018-05-29 | 2018-11-02 | 中伟新材料有限公司 | Cobalt nickel lithium manganate ternary material and preparation method thereof |
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